CN115448299A - High-conductivity graphene film and preparation method thereof - Google Patents
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Abstract
The invention discloses a high-conductivity graphene film and a preparation method thereof, and the preparation method comprises the following steps: step S1, slowly adding flake graphite into concentrated sulfuric acid, adding potassium permanganate, heating, uniformly stirring for 4 hours, dropwise adding aqueous hydrogen peroxide, carrying out heat preservation reaction until no gas is generated, dropwise adding dilute hydrochloric acid, reacting for 2 hours, dialyzing to be neutral, and filtering to prepare a graphite oxide suspension; s2, preparing a large-sheet-diameter graphene oxide film; and S3, transferring the large-sheet-diameter graphene oxide film to the surface of a quartz substrate, introducing the mixed solution into a vaporizing furnace for vaporization, preparing aniline and phenylenediamine into a mixed solution, vaporizing the mixed solution through the vaporizing furnace, introducing argon gas into the surface of the large-sheet-diameter graphene oxide, bonding amino groups and oxidation-containing groups, introducing aniline and phenylenediamine, and trimming defects generated in the preparation process of the large-sheet-diameter graphene to form a more uniform and regular form, so that the conductivity of the prepared graphene film is further improved.
Description
Technical Field
The invention belongs to the technical field of conductive materials, and particularly relates to a high-conductivity graphene film and a preparation method thereof.
Background
Transparent Conductive Films (TCFs) are currently optical transparent conductive material films that are important components of many electronic devices, including liquid crystal displays, OLEDs, touch screens, photovoltaics, and the like. TCFs for photovoltaic applications are made of inorganic and organic materials. Conventional transparent conductive materials, such as Indium Tin Oxide (ITO), are expensive, fragile, and inflexible. Although alternative networks such as carbon nanotubes, polycrystalline graphene, and metal nanowires have been proposed. Graphene is considered to be an ideal material for replacing the existing expensive ITO as a transparent conductive film most probably because of excellent conductivity, optical transparency and mechanical properties. However, for the application of the transparent conductive film, the smaller the graphene size is, the larger the resistance of the assembled transparent conductive film is, and the defects of the edges and the sheets of the graphene are formed due to the influence of ultrasound and high-speed stirring in the processing process of the graphene, so that the conductivity of the prepared conductive film is reduced.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-conductivity graphene film and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a high-conductivity graphene film comprises the following steps:
step S1, slowly adding crystalline flake graphite into concentrated sulfuric acid with the mass fraction of 70%, uniformly stirring for 30min in an ice-water bath, then adding potassium permanganate, heating to 35 ℃, uniformly stirring for 4h, slowly dropwise adding a 15% hydrogen peroxide aqueous solution after stirring, heating to 65-90 ℃, carrying out heat preservation reaction until no gas is generated, dropwise adding 5% dilute hydrochloric acid, continuously stirring and reacting for 2h, dialyzing to be neutral by using deionized water after reaction is finished, filtering to obtain graphite oxide, then adding deionized water to obtain a 1-1.5% graphite oxide suspension, and controlling the using ratio of the crystalline flake graphite, the concentrated sulfuric acid and the potassium permanganate to be 100-150 g: 2.5-3L: 30-50g, wherein the using amount of the hydrogen peroxide aqueous solution is 10% of the sum of the weight of the crystalline flake graphite and the concentrated sulfuric acid, and the using amount of the dilute hydrochloric acid is 30-50% of the volume of the hydrogen peroxide aqueous solution;
step S2, adding the graphene oxide suspension into a homogenizer, stirring for 30min at the rotating speed of 5000r/min to prepare a dispersion liquid, removing impurities, performing vacuum suction filtration by using a mixed fiber microporous filter membrane of 0.55 mu m, washing by using deionized water to form a filter membrane with a thin film on one surface, taking a PET (polyethylene terephthalate) membrane as a substrate, dropwise adding isopropanol on the surface of the substrate, attaching the surface of the thin film to the surface of a matrix, continuously dropwise adding the isopropanol until the isopropanol is wet, discharging bubbles between the filter membrane and the substrate, placing the filter membrane in a culture dish, slowly dropwise adding acetone on the surface of the filter membrane until the filter membrane is dissolved, standing for 1h, discharging the acetone, obliquely placing the substrate, respectively washing with absolute ethyl alcohol and acetone for three times, and drying to prepare a large-diameter graphene oxide thin film;
preparing graphite oxide from flake graphite by improving a Hummers method, then homogenizing at a high speed to prepare a dispersion liquid which is graphene oxide dispersion liquid, wherein ultrasonic dispersion is not adopted in the method, so that the damage of ultrasonic waves to a graphene oxide crystal structure is prevented, the sheet diameter of graphene oxide is reduced, and then preparing a large-sheet-diameter graphene oxide film through a microporous filter membrane and a PET membrane;
and S3, transferring the large-sheet-diameter graphene oxide film to the surface of a quartz substrate, placing the large-sheet-diameter graphene oxide film in a high-temperature reaction furnace, preheating to 300 ℃, arranging a vaporizing furnace in the front of the high-temperature reaction furnace, introducing the mixed solution into the vaporizing furnace for vaporization, then introducing the vaporized solution into the high-temperature reaction furnace along with argon gas flow, reacting for 30min, heating to 600 ℃, calcining for 2h to obtain the high-conductivity graphene film, controlling the temperature of the vaporizing furnace to be 280-300 ℃, introducing the mixed solution to be 3-5sccm, and controlling the flow of the argon gas flow to be 20sccm.
Further: the mixed solution in the step S3 is formed by mixing aniline and phenylenediamine according to the volume ratio of 1: 1.
A high-conductivity graphene film is prepared by the preparation method.
The invention has the beneficial effects that:
according to the invention, a high-conductivity graphene film is prepared by preparing scale graphite into graphite oxide through an improved Hummers method, then homogenizing at a high speed to prepare a dispersion liquid which is a graphene oxide dispersion liquid, ultrasonic dispersion is not adopted in the method, damage of ultrasonic waves to a graphene oxide crystal structure is prevented, the sheet diameter of the graphene oxide is reduced, then a large-sheet-diameter graphene oxide film is prepared through a microporous filter membrane and a PET film, the technical problem that the resistance of the prepared transparent conductive film is large due to small size of the graphene is solved, in addition, aniline and phenylenediamine are prepared into a mixed solution in the preparation process, vaporization is carried out through a vaporization furnace, then the surface of the large-sheet-diameter graphene oxide is introduced along with argon, amino groups are bonded with energy groups containing oxidation energy, the aniline and the phenylenediamine are introduced and can serve as carbon sources after calcination, further, defects generated in the preparation process of the large-sheet-diameter graphene are trimmed, a more uniform and regular form is formed, and further the conductivity of the prepared graphene film is further improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a high-conductivity graphene film comprises the following steps:
step S1, slowly adding flake graphite into concentrated sulfuric acid with the mass fraction of 70%, uniformly stirring for 30min in an ice water bath, then adding potassium permanganate, heating to 35 ℃, uniformly stirring for 4h, slowly dropwise adding a 15% hydrogen peroxide aqueous solution with the mass fraction after stirring is finished, heating to 65 ℃, carrying out heat preservation reaction until no gas is generated, dropwise adding a 5% dilute hydrochloric acid, continuously stirring and reacting for 2h, dialyzing to be neutral by using deionized water after the reaction is finished, filtering to obtain graphite oxide, then adding deionized water to obtain a 1% graphite oxide suspension, controlling the dosage ratio of the flake graphite, the concentrated sulfuric acid and the potassium permanganate to be 100 g: 2.5L: 30g, the dosage of the hydrogen peroxide aqueous solution to be 10% of the sum of the weight of the flake graphite and the concentrated sulfuric acid, and the dosage of the dilute hydrochloric acid to be 30% of the volume of the hydrogen peroxide aqueous solution;
step S2, adding the graphene oxide suspension into a homogenizer, stirring for 30min at the rotating speed of 5000r/min to prepare a dispersion liquid, removing impurities, performing vacuum suction filtration by using a mixed fiber microporous filter membrane of 0.55 mu m, washing by using deionized water to form a filter membrane with a thin film on one surface, taking a PET (polyethylene terephthalate) membrane as a substrate, dropwise adding isopropanol on the surface of the substrate, attaching the surface of the thin film to the surface of a matrix, continuously dropwise adding the isopropanol until the isopropanol is wet, discharging bubbles between the filter membrane and the substrate, placing the filter membrane in a culture dish, slowly dropwise adding acetone on the surface of the filter membrane until the filter membrane is dissolved, standing for 1h, discharging the acetone, obliquely placing the substrate, respectively washing with absolute ethyl alcohol and acetone for three times, and drying to prepare a large-diameter graphene oxide thin film;
and S3, transferring the large-sheet-diameter graphene oxide film to the surface of a quartz substrate, placing the large-sheet-diameter graphene oxide film in a high-temperature reaction furnace, preheating to 300 ℃, arranging a vaporizing furnace in the front of the high-temperature reaction furnace, introducing the mixed solution into the vaporizing furnace for vaporization, then introducing the vaporized solution into the high-temperature reaction furnace along with argon gas flow, reacting for 30min, heating to 600 ℃, calcining for 2h to obtain the high-conductivity graphene film, controlling the temperature of the vaporizing furnace to be 280 ℃, introducing the mixed solution to be 3sccm, controlling the flow of the argon gas flow to be 20sccm, and mixing aniline and phenylenediamine according to the volume ratio of 1: 1 to obtain the mixed solution.
Example 2
A preparation method of a high-conductivity graphene film comprises the following steps:
step S1, slowly adding flake graphite into concentrated sulfuric acid with the mass fraction of 70%, uniformly stirring for 30min in an ice water bath, then adding potassium permanganate, heating to 35 ℃, uniformly stirring for 4h, slowly dropwise adding a 15% hydrogen peroxide aqueous solution with the mass fraction after stirring is finished, heating to 75 ℃, carrying out heat preservation reaction until no gas is generated, dropwise adding a 5% dilute hydrochloric acid, continuously stirring and reacting for 2h, dialyzing to be neutral by deionized water after the reaction is finished, filtering to obtain graphite oxide, then adding deionized water to obtain a 1.2% graphite oxide suspension, controlling the dosage ratio of the flake graphite, the concentrated sulfuric acid and the potassium permanganate to be 120 g: 2.8L: 40g, controlling the dosage of the hydrogen peroxide aqueous solution to be 10% of the sum of the weight of the flake graphite and the concentrated sulfuric acid, and controlling the dosage of the dilute hydrochloric acid to be 35% of the volume of the hydrogen peroxide aqueous solution;
step S2, adding the graphene oxide suspension into a homogenizer, stirring for 30min at the rotating speed of 5000r/min to prepare a dispersion liquid, removing impurities, performing vacuum suction filtration by using a mixed fiber microporous filter membrane of 0.55 mu m, washing by using deionized water to form a filter membrane with a thin film on one surface, taking a PET (polyethylene terephthalate) membrane as a substrate, dropwise adding isopropanol on the surface of the substrate, attaching the surface of the thin film to the surface of a matrix, continuously dropwise adding the isopropanol until the isopropanol is wet, discharging bubbles between the filter membrane and the substrate, placing the filter membrane in a culture dish, slowly dropwise adding acetone on the surface of the filter membrane until the filter membrane is dissolved, standing for 1h, discharging the acetone, obliquely placing the substrate, respectively washing with absolute ethyl alcohol and acetone for three times, and drying to prepare a large-diameter graphene oxide thin film;
and S3, transferring the large-sheet-diameter graphene oxide film to the surface of a quartz substrate, placing the quartz substrate in a high-temperature reaction furnace, preheating to 300 ℃, arranging a vaporization furnace in the front of the high-temperature reaction furnace, introducing the mixed solution into the vaporization furnace for vaporization, then introducing the vaporized solution into the high-temperature reaction furnace along with argon gas flow, reacting for 30min, heating to 600 ℃, and calcining for 2h to obtain the high-conductivity graphene film, wherein the temperature of the vaporization furnace is controlled to be 300 ℃, the introduction amount of the mixed solution is 4sccm, the flow rate of the argon gas flow is 20sccm, and the mixed solution is formed by mixing aniline and phenylenediamine according to the volume ratio of 1: 1.
Example 3
A preparation method of a high-conductivity graphene film comprises the following steps:
step S1, slowly adding crystalline flake graphite into concentrated sulfuric acid with the mass fraction of 70%, uniformly stirring in an ice-water bath for 30min, then adding potassium permanganate, heating to 35 ℃, uniformly stirring for 4h, slowly dropwise adding a 15% aqueous hydrogen peroxide solution after stirring, heating to 85 ℃, carrying out heat preservation reaction until no gas is generated, dropwise adding dilute hydrochloric acid with the mass fraction of 5%, continuously stirring and reacting for 2h, dialyzing to be neutral by deionized water after the reaction is finished, filtering to obtain graphite oxide, then adding deionized water to obtain a 1.4% graphite oxide suspension, controlling the dosage ratio of the crystalline flake graphite, the concentrated sulfuric acid and the potassium permanganate to be 140 g: 2.8L: 45g, controlling the dosage of the aqueous hydrogen peroxide solution to be 10% of the sum of the weight of the crystalline flake graphite and the concentrated sulfuric acid, and the dosage of the dilute hydrochloric acid to be 40% of the volume of the aqueous hydrogen peroxide solution;
step S2, adding the graphene oxide suspension into a homogenizer, stirring for 30min at the rotating speed of 5000r/min to prepare a dispersion liquid, removing impurities, performing vacuum suction filtration by using a mixed fiber microporous filter membrane of 0.55 mu m, washing by using deionized water to form a filter membrane with a thin film on one surface, taking a PET (polyethylene terephthalate) membrane as a substrate, dropwise adding isopropanol on the surface of the substrate, attaching the surface of the thin film to the surface of a matrix, continuously dropwise adding the isopropanol until the isopropanol is wet, discharging bubbles between the filter membrane and the substrate, placing the filter membrane in a culture dish, slowly dropwise adding acetone on the surface of the filter membrane until the filter membrane is dissolved, standing for 1h, discharging the acetone, obliquely placing the substrate, respectively washing with absolute ethyl alcohol and acetone for three times, and drying to prepare a large-diameter graphene oxide thin film;
and S3, transferring the large-sheet-diameter graphene oxide film to the surface of a quartz substrate, placing the large-sheet-diameter graphene oxide film in a high-temperature reaction furnace, preheating to 300 ℃, arranging a vaporizing furnace in the front of the high-temperature reaction furnace, introducing the mixed solution into the vaporizing furnace for vaporization, then introducing the vaporized solution into the high-temperature reaction furnace along with argon gas flow, reacting for 30min, heating to 600 ℃, calcining for 2h to obtain the high-conductivity graphene film, controlling the temperature of the vaporizing furnace to be 300 ℃, introducing the mixed solution to be 5sccm, controlling the flow of the argon gas flow to be 20sccm, and mixing aniline and phenylenediamine according to the volume ratio of 1: 1 to obtain the mixed solution.
Example 4
A preparation method of a high-conductivity graphene film comprises the following steps:
step S1, slowly adding crystalline flake graphite into concentrated sulfuric acid with the mass fraction of 70%, uniformly stirring for 30min in an ice water bath, then adding potassium permanganate, heating to 35 ℃, uniformly stirring for 4h, slowly dropwise adding a 15% hydrogen peroxide aqueous solution after stirring is finished, heating to 90 ℃, carrying out heat preservation reaction until no gas is generated, dropwise adding a 5% dilute hydrochloric acid, continuously stirring and reacting for 2h, dialyzing to be neutral by using deionized water after the reaction is finished, filtering to obtain graphite oxide, then adding deionized water to obtain a 1.5% graphite oxide suspension, controlling the dosage ratio of the crystalline flake graphite, the concentrated sulfuric acid and the potassium permanganate to be 150 g: 3L: 50g, the dosage of the hydrogen peroxide aqueous solution to be 10% of the sum of the weight of the crystalline flake graphite and the concentrated sulfuric acid, and the dosage of the dilute hydrochloric acid to be 50% of the volume of the hydrogen peroxide aqueous solution;
step S2, adding the graphene oxide suspension into a homogenizer, stirring for 30min at the rotating speed of 5000r/min to prepare a dispersion liquid, removing impurities, performing vacuum suction filtration by using a mixed fiber microporous filter membrane of 0.55 mu m, washing by using deionized water to form a filter membrane with a thin film on one surface, taking a PET (polyethylene terephthalate) membrane as a substrate, dropwise adding isopropanol on the surface of the substrate, attaching the surface of the thin film to the surface of a matrix, continuously dropwise adding the isopropanol until the isopropanol is wet, discharging bubbles between the filter membrane and the substrate, placing the filter membrane in a culture dish, slowly dropwise adding acetone on the surface of the filter membrane until the filter membrane is dissolved, standing for 1h, discharging the acetone, obliquely placing the substrate, respectively washing with absolute ethyl alcohol and acetone for three times, and drying to prepare a large-diameter graphene oxide thin film;
and S3, transferring the large-sheet-diameter graphene oxide film to the surface of a quartz substrate, placing the quartz substrate in a high-temperature reaction furnace, preheating to 300 ℃, arranging a vaporization furnace in the front of the high-temperature reaction furnace, introducing the mixed solution into the vaporization furnace for vaporization, then introducing the vaporized solution into the high-temperature reaction furnace along with argon gas flow, reacting for 30min, heating to 600 ℃, and calcining for 2h to obtain the high-conductivity graphene film, wherein the temperature of the vaporization furnace is controlled to be 300 ℃, the introduction amount of the mixed solution is 5sccm, the flow rate of the argon gas flow is 20sccm, and the mixed solution is formed by mixing aniline and phenylenediamine according to the volume ratio of 1: 1.
Comparative example 1
The comparative example is a conductive graphene film prepared in patent application CN 2017114155105.
Comparative example 2
The present comparative example is a conductive graphene film prepared in patent CN 2019101046486.
Comparative example 3
This comparative example is a graphene conductive film produced by a technology company of yowa.
The performance of the conductive graphene films prepared in examples 1 to 4 and comparative examples 1 to 3 was measured, and the results are shown in the following table, and the test methods were as follows:
the light transmittance was measured by UV-Vis, and the resistance of the conductive film was measured by the four-probe method.
As can be seen from the above table, the conductive films prepared in examples 1 to 4 of the present invention have high conductivity and better light transmittance.
The foregoing is illustrative and explanatory only of the present invention, and it is intended that the present invention cover modifications, additions, or substitutions by those skilled in the art, without departing from the spirit of the invention or exceeding the scope of the claims.
Claims (5)
1. A preparation method of a high-conductivity graphene film is characterized by comprising the following steps: the method comprises the following steps:
step S1, slowly adding crystalline flake graphite into concentrated sulfuric acid with the mass fraction of 70%, uniformly stirring in an ice-water bath for 30min, then adding potassium permanganate, heating to 35 ℃, uniformly stirring for 4h, slowly dropwise adding a 15% hydrogen peroxide aqueous solution after stirring, heating to 65-90 ℃, carrying out heat preservation reaction until no gas is generated, dropwise adding a 5% dilute hydrochloric acid, continuously stirring and reacting for 2h, dialyzing with deionized water to neutrality after the reaction is finished, filtering to obtain graphite oxide, and then adding deionized water to obtain a 1-1.5% graphite oxide suspension;
step S2, adding the graphene oxide suspension into a homogenizer, stirring for 30min at the rotating speed of 5000r/min to prepare a dispersion liquid, then performing vacuum suction filtration by using a fiber-mixed microporous filter membrane of 0.55 mu m, washing with deionized water to form a filter membrane with a thin film on one surface, taking a PET (polyethylene terephthalate) membrane as a substrate, dropwise adding isopropanol on the surface of the substrate, attaching the surface of the membrane to the surface of a matrix, continuously dropwise adding the isopropanol, discharging bubbles between the filter membrane and the substrate, placing the membrane in a culture dish, slowly dropwise adding acetone on the surface of the filter membrane until the filter membrane is dissolved, standing for 1h, discharging the acetone, obliquely placing the substrate, respectively cleaning with absolute ethyl alcohol and acetone for three times, and drying to prepare the large-diameter graphene oxide film;
and S3, transferring the large-sheet-diameter graphene oxide film to the surface of a quartz substrate, placing the large-sheet-diameter graphene oxide film in a high-temperature reaction furnace, preheating to 300 ℃, arranging a vaporizing furnace in the front of the high-temperature reaction furnace, introducing the mixed solution into the vaporizing furnace for vaporization, then introducing the vaporized solution into the high-temperature reaction furnace along with argon gas flow, reacting for 30min, heating to 600 ℃, and calcining for 2h to obtain the high-conductivity graphene film.
2. The method for preparing the highly conductive graphene film according to claim 1, wherein: in the step S1, the dosage ratio of the crystalline flake graphite, the concentrated sulfuric acid and the potassium permanganate is controlled to be 100-150 g: 2.5-3L: 30-50g, the dosage of the aqueous hydrogen peroxide solution is 10% of the sum of the weight of the crystalline flake graphite and the concentrated sulfuric acid, and the dosage of the dilute hydrochloric acid is 30-50% of the volume of the aqueous hydrogen peroxide solution.
3. The method for preparing the highly conductive graphene film according to claim 1, wherein: in the step S3, the temperature of the vaporization furnace is controlled to be 280-300 ℃, the introduction amount of the mixed solution is 3-5sccm, and the flow rate of the argon gas flow is 20sccm.
4. The method for preparing the highly conductive graphene film according to claim 1, wherein: the mixed solution in the step S3 is formed by mixing aniline and phenylenediamine according to the volume ratio of 1: 1.
5. A highly conductive graphene film, comprising: the preparation method of claim 1.
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| WO2024037662A1 (en) * | 2022-08-18 | 2024-02-22 | 楚隆市场策划有限公司 | Preparation method for and use of bismuth ion filter membrane |
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